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2-(3-Nitropyridin-4-yl)ethanol → 4-Pyridineethanol, 3-amino-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(3-Nitropyridin-4-yl)ethanol | HCID 59547366 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | HCID 178418361 | HCID 178418361 | — |
| 生成物 | 4-Pyridineethanol, 3-amino- | HCID 46835596 | 81% |
反応手順
2-(3-Nitropyridin-4-yl)ethanol (15) (WO 2006136562) (2.00 g, 11.89 mmol) in MeOH (150 mL) was passed through a Thales H-cube at 2.0 mL·min−1 using Pd/C Cat-Cart (55 mm) in controlled mode at 30° C., 30 bar. Analysis by LC-MS showed a significant amount of starting material was still present. The solution was passed through the H-cube a second time at 2.0 mL·min−1 in full hydrogen mode at RT, and again at 2.0 mL·min−1 in full hydrogen mode at 40° C. Evaporation of the volatiles gave 2-(3-Aminopyridin-4-yl)ethanol (16) as a purple oil (1.30 g, 81%): m/z 139 (M+H)+ (ES+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08293748B2 |
| 出典データセット | uspto-grants-2012_10 |
| ORD ID | ord-6aa2ab494b594ecd9c23e01fbde86180 |
| 出典メモ | uspto-grants-2012_10 |